Instrumentation Preparation and characterization of catalyst Catalyst testing and analysis of prod- uct

Bulletin of Chemical Reaction Engineering Catalysis, 12 2, 2017, 220 Copyright © 2017, BCREC, ISSN 1978-2993 weight and viscosity should be lowered. To lower the molecular weight, viscosity, and aro- matics content, the coal tar must be processed by hydrogenation and cracking or hydrocrack- ing. The cracking process requires a catalyst that has dual functions, i.e. metal component as the hydrogenation catalyst and acid compo- nent as the cracking catalyst [3]. Ones of the transition metals that most commonly used in the hydrocracking process are Co and Mo. Meanwhile, the most common catalyst used in catalytic cracking and hydrocracking is zeolite [4-10]. Wang et al. [11] has done a research using zeolite catalyst, that reaction initially took place at high temperature without a catalyst, but when using a catalyst, the reaction could take place at lower temperature. Research by Emelik [12] and Tsitsishvili [13] about the effect of Ni and Mo metals showed that catalyst with Ni and Mo required higher specific surface area to produce greater distribution of Mo. Anggoro et al. [14] and Zeno [15] studied the effect of Co and Mo metals addition on Y zeolite and found that at higher concentration of the metal, the catalyst acidity was higher if sup- ported by equitable distribution. Therefore, in this research, the Co and Mo impregnated into Y zeolite was applied to convert coal tar into liquid fuels. The effect of impregnation temperature and time need to be considered to determine the best preparation of Co-MoY zeolite condition which can be used as a hydrocracking catalyst of coal tar. This has encouraged research to de- termine the effect of impregnation condition of Co and Mo into Y zeolite in coal tar hydrocrack- ing into liquid fuel. Therefore, the objectives of this research are to determine the effect of tem- perature and length time of impregnation on the preparation of the Co-MoY zeolite catalyst, to characterize the Co-MoY zeolite catalyst, and to test the catalyst on the conversion of coal tar to liquid fuel. 2. Materials and Method 2.1. Materials The materials used were a coal tar from PT. Sango Ceramic Indonesia, Y-zeolite 99.9 and ZSM-5 99.9 from Zeolyst International, CoNO 3 2 .6H 2 O 99.0 from Merck, NH 4 6 Mo 7 O 24 .4H 2 O 99.3 from Merck, ammonia from Merck, and hydrogen gas 99.99 from PT. Aneka Gas.

2.2. Instrumentation

The functional group detection of the cata- lysts was analyzed by Fourier Transform Infra Red FTIR Shimadzu IR Prestige-21. The crys- tallinity of catalyst and its structure were done by X-Ray Diffraction XRD Shimadzu XRD- 7000, and the total acidity determination was conducted using method of ammonia adsorption gravimetrically. The liquid fuel product was analyzed using Gas Chromatogra- phy.

2.3. Preparation and characterization of catalyst

The Co-MoY zeolite catalyst was prepared using impregnation method. Five grams of Y zeolite, cobalt metal obtained from CoNO 3 2 .6H 2 O 0.985 grams, and molybdenum metal from NH 4 6 Mo 7 O 24 .4H 2 O 4.34 grams were dissolved in 50 mL of distilled water. The solution was then heated to temperature as stated in independent variables and stirred for the length time as stated in the variables Table 1. Thus, the samples were filtered us- ing a vacuum pump until no more water was dripping. Further, the samples were dried in an oven at temperature of 100 °C for 24 hours. The dried samples were then calcined at tem- perature of 550 °C for 3 hours. The functional group of the catalysts was analyzed by FT-IR method. The stability of catalyst structure was analyzed by X-Ray Diffraction. The total acid- ity of catalysts was determined using the am- monia gravimetrically method [16].

2.4. Catalyst testing and analysis of prod- uct

Hydrocracking process was performed in a 1000 mL three-neck flask size as a place of coal tar 100 mL, evaporated using a hot plate 300 Run Temperature °C Time minutes 1 35 10 2 35 30 3 55 10 4 55 30 5 31 20 6 59 20 7 45 6 8 45 34 9 45 20 10 45 20 Table 1. Matrix of experimental design Bulletin of Chemical Reaction Engineering Catalysis, 12 2, 2017, 221 Copyright © 2017, BCREC, ISSN 1978-2993 o C, and completed with a magnetic stirrer. Hy- drogen gas used as the reactant gas of the hy- drocracking. The reactor used was a stainless steel tube reactor completed with ceramic and glass wool in order to support position of the catalyst as shown Figure 1. There were a tem- perature indicator and a heater in the reactor, so the temperature reaction was maintained at 350 °C. Seven grams of catalyst, consisted of 5 grams catalyst which had been prepared Co- MoY zeolite and 2 grams ZSM-5 catalyst, was put in the reactor tube. The cooling system of the reactor used a condenser and ethylene gly- col as coolant. Length time of the hydrocrack- ing reaction was 1 hour. 3. Results and Discussion 3.1. Catalyst characterization using FTIR